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Poly (cyclopentadiene-dicyclopentadiene) copolymer and synthesis method thereof

A technology of dicyclopentadiene and cyclopentadiene, applied in the field of poly(cyclopentadiene-dicyclopentadiene) copolymer and its synthesis, to achieve the effect of improving the index of elasticity and toughness

Inactive Publication Date: 2011-11-09
青岛德明力兴新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no research on the application of cyclopentadiene in ring-opening metathesis copolymerization.

Method used

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  • Poly (cyclopentadiene-dicyclopentadiene) copolymer and synthesis method thereof
  • Poly (cyclopentadiene-dicyclopentadiene) copolymer and synthesis method thereof
  • Poly (cyclopentadiene-dicyclopentadiene) copolymer and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 0.5mmol of tungsten hexachloride and 10mmol of triisobutylaluminum to a 150ml sealed tube under nitrogen protection, mix well and then add 40ml of toluene.

[0045] After mixing evenly, aging at 30° C. for 1 hour to form a purple-black heterogeneous solution.

[0046] Add 40ml cyclohexane, 0.06mol cyclopentadiene and 0.09mol dicyclopentadiene to a 250ml dry polymerization bottle under nitrogen protection, mix well and then add 80ml cyclohexane to mix;

[0047] Then, 6.7 ml of the catalyst solution prepared above was added. After mixing evenly, polymerize at room temperature for 3 hours;

[0048] Subsequently, an appropriate amount of ethanol solution containing anti-aging agent 264 was added to terminate the reaction, washed with distilled water, and dried in a vacuum oven at 60°C until constant weight.

[0049] The obtained copolymer number average molecular weight (M n ) is 3.7×10 4 g / mol, molecular weight distribution index (M w / M n ) is 5.2.

Embodiment 2

[0051] Under nitrogen protection, 0.5 mmol of molybdenum pentachloride and 2.5 mmol of aluminum trichloride were added to a 150 ml sealed tube. The aging method was used to prepare the catalyst according to the method in Example 1. After aging, a blue-purple heterogeneous solution was obtained.

[0052] Add 0.12mol cyclopentadiene and 0.06mol dicyclopentadiene to a 250ml dry polymerization bottle under nitrogen protection;

[0053] After mixing evenly, 120ml of cyclohexane was added, and then mixed evenly, and then 5.8ml of the prepared catalyst solution was added.

[0054] After mixing evenly, polymerize at room temperature for 8 hours, then add an appropriate amount of ethanol solution containing anti-aging agent 264 to terminate the reaction, wash with distilled water and dry in a vacuum oven at 60°C until constant weight.

[0055] Gained copolymer has certain elasticity, number average molecular weight (M n ) is 15.6×10 4 g / mol, molecular weight distribution index (M w ...

Embodiment 3

[0057] Add 0.5mmol tungsten hexachloride and 0.25mmol aluminum tribromide to the 150ml sealed tube under the protection of nitrogen, and prepare the catalyst according to the method in Example 1 for the aging method. After aging, it becomes a blue-violet heterogeneous solution.

[0058] Add 0.172mol cyclopentadiene and 0.01mol dicyclopentadiene to a 250ml dry polymerization bottle under the protection of nitrogen, mix well, then add 90ml cyclohexane, mix well, then add the prepared catalyst solution 16.2ml. After mixing evenly, place in a 10°C water bath to polymerize for 6 hours;

[0059] Then add an appropriate amount of ethanol solution containing anti-aging agent 264 to terminate the reaction, wash with distilled water and dry in a vacuum oven at 60°C until constant weight.

[0060] The obtained copolymer number average molecular weight (M n ) is 9.5×10 3 g / mol, molecular weight distribution index (M w / M n ) is 6.2.

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Abstract

The invention discloses a poly (cyclopentadiene-dicyclopentadiene) copolymer and a synthesis method thereof. Cyclopentadiene and dicyclopentadiene which are taken as polymerization monomers are subjected to ring-opening metathesis copolymerization to form a novel high polymer material. By adjusting the rate of the dicyclopentadiene in the comonomers, the content of a fat ring chain structure in the poly (cyclopentadiene-dicyclopentadiene) copolymer is adjusted, so that various high polymer materials with different properties and purposes are synthesized. Moreover, the dicyclopentadiene is used as one of the monomers and applied to preparing rubber materials, and a monomer ratio of the cyclopentadiene to the dicyclopentadiene is adjusted, so that the generated random copolymer has higher number-average molecular weight and proper Mooney viscosity.

Description

technical field [0001] The present invention relates to a kind of poly(cyclopentadiene-dicyclopentadiene) copolymer and its synthetic method for making rubber, plastics or other macromolecular materials, specifically cyclopentadiene and dicyclopentadiene are used as Monomers undergo ring-opening metathesis polymerization to form random copolymers. Background technique [0002] According to the understanding and application of the current prior art, in the ring-opening metathesis polymerization of cycloolefins, the carbon-carbon double bonds of the monomers are continuously metathesized to open the ring, with the number, bonding sequence and bond type of methylene and double bonds characteristics that do not change. [0003] In addition, the cis-trans configuration of the product and its ratio can also be adjusted with the type of catalyst. [0004] The ring-opening metathesis reaction usually uses a two-component catalyst, namely MtX n / MR n x 3-n , where Mt is tungsten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/08
Inventor 王浩何丽霞王继叶张修农
Owner 青岛德明力兴新材料股份有限公司
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